CN103646772B - A kind of preparation method of R-Fe-B based sintered magnet - Google Patents
A kind of preparation method of R-Fe-B based sintered magnet Download PDFInfo
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- CN103646772B CN103646772B CN201310596041.7A CN201310596041A CN103646772B CN 103646772 B CN103646772 B CN 103646772B CN 201310596041 A CN201310596041 A CN 201310596041A CN 103646772 B CN103646772 B CN 103646772B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 103
- 238000000034 method Methods 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 21
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 239000008187 granular material Substances 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 12
- 239000003921 oil Substances 0.000 claims abstract description 8
- 238000005554 pickling Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 14
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 9
- 229910052771 Terbium Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000007796 conventional method Methods 0.000 abstract 1
- 239000003643 water by type Substances 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 20
- 239000002994 raw material Substances 0.000 description 10
- 150000002910 rare earth metals Chemical class 0.000 description 9
- 230000005389 magnetism Effects 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000012466 permeate Substances 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000001883 metal evaporation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000010183 spectrum analysis Methods 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- 235000011149 sulphuric acid Nutrition 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Manufacturing Cores, Coils, And Magnets (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to the preparation method of a kind of R Fe B based sintered magnet, initially with conventional method R Fe B based sintered magnet, through steps such as oil removing, pickling, deionized waters, sintered magnet is cleaned；Secondly, being paved with metal Dy bottom magazine, shape does not limits, and then fills up zirconium oxide, silicon dioxide or alumina powder in magazine；Again above-mentioned sintered magnet is inserted in powder along the direction that magnetizing direction is vertical, or, according to metal Dy plate, high-melting-point powder particle, sintered magnet, the order of high-melting-point powder particle during stratiform is placed in magazine successively, magnet bottom does not contacts with the Dy granule bottom magazine, and does not contacts between adjacent magnets；Finally, magazine is put into sintering furnace, under vacuum or Ar gas shielded atmosphere, 750～1000 DEG C carry out heat treatment, make Dy pass through to spread and enter inside sintered magnet along crystal boundary.The present invention greatly reduces the processing cost of Dy, simplifies technique, and after heat treatment, magnet coercivity increases substantially.
Description
Technical field
The present invention relates to the preparation method of a kind of R-Fe-B based sintered magnet, belong to rare earth permanent-magnetic material neck
Territory.
Background technology
Owing to having excellent magnetic property, R-Fe-B based sintered magnet has just been widely used since invention
In information industry, automobile industry, power equipment, household electrical appliance, petrochemical industry, machine-building, aviation
The field such as space flight, medical machinery.
Over the past two years, due to the fluctuation of the rare earth prices of raw materials, especially heavy rare earth prices of raw materials experience
After jumping up, rare-earth magnet client an urgent demand rare-earth magnet supplier uses new technology, reduces
The raw-material usage amount of heavy rare earth, reduces cost；Many rare-earth magnet clients have begun to consider use valency
The ferrimagnet that lattice are the cheapest replaces the part neodymium iron boron magnetic body being previously used.
Coercivity is the important parameter weighing magnet magnetic property.It is dilute that traditional method adds weight in fusion process
Soil raw material can improve the coercivity of magnet, but theoretical proof, and heavy rare earth element is only distributed in crystalline substance
Forming Nd-rich phase in boundary, the rotation of suppression domain just can significantly improve the coercivity of magnet；And melting
Journey major part heavy rare earth element enters principal phase, causes heavy rare earth element utilization rate the lowest.
Grain boundary decision method refers to arrange heavy rare earth element around sintered magnet, at high temperature makes heavy rare earth unit
Element is constantly replaced with Grain-Boundary Phase, burns so that heavy rare earth element enters only along principal phase grain boundary decision
Knot method within magnet.Use the method can be substantially reduced the usage amount of heavy rare earth element, significantly carry
The magnetic property of high magnet.
Patent documentation CN-200610064800.5 discloses following method: by R (Dy or Tb)
Oxide, fluoride or oxyfluoride mix with ethanol after make slurry, be evenly applied to sinter magnetic
Surface, carries out heat treatment to magnet afterwards, makes the R in compound and the Pr in sintered magnet crystal boundary
Or Nd replaces, and make heavy rare earth element R to sintered magnet diffusion inside, thus magnetic is greatly improved
The coercivity of body.
Patent documentation JP-A 2,006 344782 discloses following method: put into very by sintered magnet
Reason indoor, vacancy, at least one evaporation material of configuration Dy or Tb in process chamber, heating makes evaporation material
Evaporation, is diffused in sintered magnet Grain-Boundary Phase before forming film on sintered magnet surface.
Patent documentation CN-200610064800.5 uses the oxidation of heavy rare earth element R (Dy or Tb)
Thing, fluoride or oxyfluoride, bury sintered magnet and carry out heat-treating methods the most afterwards.Use
During the method, when Pr, Nd element in crystal boundary occurs displacement mutually with heavy rare earth, powder forms Pr
Or the oxide of Nd, fluoride and oxyfluoride.Therefore, the concentration of the R in compound powder
Reduce along with the increase of powder access times, thus treatment effect can worse and worse, the coercivity of magnet
Increasing can be more and more lower, thus causes the powder access times of heavy rare earth element R limited, thus adds
Raw-material cost.
Patent documentation JP-A 2,006 344782 uses the steam of heavy rare earth element R (Dy or Tb)
Evaporate under vacuum high-temperature, the method diffusing into sintered magnet.Use the method time, sintered magnet with
Heavy rare earth element R can not directly contact, and sintered magnet is placed on support or other supporters.When weight
When the steam of rare earth element and Grain-Boundary Phase react, Grain-Boundary Phase is in molten condition, under this condition,
The place that sintered magnet contacts with support or supporter deforms due to the action of gravity of magnet itself, cold
But after, on sintered magnet, there is pit contact site, and is sticked together with support or supporter.Therefore,
Use the method to being subject to processing sintered magnet composition, heat treatment temperature, heat-treatment furnace atmosphere and supporter material
Material has strict demand, and controllability is poor.
Summary of the invention
The present invention is the new method designed for solving the problems referred to above, due to the vacuum and steam pressure relatively Dy of Tb
Much lower, after process, magnet performance promotes inconspicuous, thus the method for the present invention is only limitted to metal Dy, its
Purpose is to improve raw-material utilization rate, ensures not produce contact pit and vestige on magnet simultaneously,
Reduce cost on the basis of improving sintered magnet magnetic property, improve magnet outward appearance.
In order to solve problems of the prior art, the present invention provides a kind of R-Fe-B based sintered magnet
Preparation method, including:
1) R is prepared1-Fe-B-M sintered magnet, wherein, R1Selected from Nd, Pr, Dy, Tb, Ho, Gd
In one or several, its total amount is 26wt%～33wt%；M selected from Ti, V, Cr, Mn, Co,
One or several in Ni, Ga, Ca, Cu, Zn, Si, Al, Mg, Zr, Nb, Hf, Ta, W, Mo
Kind, its total amount is 0～5wt%；B total amount is 0.5wt%～2wt%；Remaining is Fe；
2) by step 1) sintered magnet that obtains carries out at oil removing, pickling, activation and deionized water cleaning
Reason；
3) by step 2) in clean after sintered magnet be inserted into along the direction vertical with magnetizing direction and fill out
Have in the magazine of high-melting-point powder particle, wherein first at magazine before filling described high-melting-point powder particle
Bottom is paved with metal Dy；Or, according to metal Dy plate, high-melting-point powder particle, sintered magnet, height
The order of fusing point powder particle is during stratiform is placed in magazine successively, wherein sintered magnet magnetizing direction and magazine
Short transverse is parallel；
4) by step 3) in hold the magazine of sintered magnet, high-melting-point powder particle and metal Dy and put into
In vacuum sintering furnace, heat treatment 2～72h in 750～1000 DEG C, vacuum degree control in vacuum sintering furnace
10-2～10-5Use the Ar protective atmosphere of 5～20kPa in Pa or vacuum sintering furnace, make metal Dy
Steam is entered inside sintered magnet by grain boundary decision；
5) by step 4) process after sintered magnet in 450～600 DEG C of Ageing Treatment 1～10h, obtain
R-Fe-B based sintered magnet.
Wherein, Fe is ferrum, and B is boron.R1-Fe-B-M sintered magnet is from R1At-Fe-B-M alloy processing
Reason obtains, R1, M as a kind of component of alloy, can choose from disclosed element any one or
Multiple.On the basis of technique scheme, the present invention can also do following improvement.
Preferably, in described step 3) in, when sintered magnet is inserted along the direction vertical with magnetizing direction
When entering in the magazine be filled with high-melting-point powder particle, the height of the described high-melting-point powder particle of interpolation exists
The height on direction that sintered magnet is vertical with magnetizing direction is set to ensure that magnet can be completely buried in institute
State in high-melting-point powder particle.
Preferably, in described step 3) in, when sintered magnet is inserted along the direction vertical with magnetizing direction
When entering in the magazine be filled with high-melting-point powder particle, sintered magnet not with magazine bottom metal bed material connect
Touch, do not contact each other between sintered magnet simultaneously.
Preferably, in described step 3) in, when according to metal Dy plate, high-melting-point powder particle, sintering
When magnet, the order of high-melting-point powder particle are during stratiform is placed in magazine successively, the described high-melting-point of interpolation
The thickness of powder particle is 1～50mm.
Preferably, the thickness of the described high-melting-point powder particle of interpolation is 1～20mm.
It is furthermore preferred that described high-melting-point powder particle is zirconium oxide, silicon dioxide or alumina powder
Any one in Li, particle diameter is between 50～5000 μm.
Preferably, described step 3) in the described metal Dy bed material that is paved with bottom magazine be tabular,
Granular or powder.
Preferably, in described step 4) in, vacuum-sintering in-furnace temperature is 800～950 DEG C, heat treatment
Time is 5～72h, and in vacuum sintering furnace, vacuum is 10-3～10-4Pa；Or adopt in vacuum sintering furnace
With the Ar protective atmosphere of 5～10kPa.
Preferably, in described step 5) in, described aging temperature is 470～550 DEG C, during process
Between be 2～5h.
The invention has the beneficial effects as follows:
Method used according to the invention, geomery and the size of heavy metal raw material Dy no longer have sternly
The requirement of lattice, it is possible to use tabular, graininess or powdery, thus reduce raw material processing cost；
Being inserted directly in powder by sintered magnet, heavy metal steam is by zirconium oxide, silicon dioxide or aluminium oxide
Powder voids arrives sintered magnet surface, and vapour concentration is uniform, and after process, the homogeneity of sintered magnet is good；
High-melting-point powder particle does not reacts with Dy steam generation, and reusing is good；Due to sintered magnet not with
Support or supporter contact, will not just produce contact pit and vestige, and after process, sintered magnet outward appearance is bright
Aobvious improvement.
Accompanying drawing explanation
Fig. 1 is that sintered magnet directly contacts, with support or supporter, the explanatory diagram sticked together.
Fig. 2 is the explanatory diagram fed in magazine in the present invention.
Fig. 3 is the explanatory diagram that in the present invention, in magazine, another kind feeds.
In accompanying drawing, the content representated by each label is as follows:
1, magazine lid, 2, magazine, 3, sintered magnet, 4, zirconium oxide, silicon dioxide or oxidation
Aluminium powder particle, 5, metal Dy bed material, 6, magazine lid, 7, magazine, 8, sintered magnet, 9, oxygen
Change zirconium, silicon dioxide or alumina powder granule, 10, metal Dy plate, 11, sintered magnet, 12,
Support or supporter, 13, before non-heat treated at non-adhesion, 14, at heat treated posterior synechiae.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, and
Non-for limiting the scope of the present invention.
The sintered magnet that is subject to processing used in the present invention can use following methods to prepare:
First, sintering briquette alloy, by vacuum or noble gas, typically melts metal in argon gas atmosphere
Or alloy raw material, start cast 1300～1600 DEG C of temperature, more excellent is 1400～1500 DEG C；And
Will in melt cast to chilling roller formed scale, sharp cooling roll rotating speed is 20～60r/min, more excellent be 30～
50r/min, logical cooling water in chilling roller；Secondly, scale, through HD powder process, airflow milling, makes granularity
Being the powder of 2～10 μm, more excellent is 3～5 μm；Thirdly, orientation compacting in the magnetic field of 15KOe
Molding；Thirdly, green compact are placed in the sintering furnace under Ar atmosphere, at 900～1300 DEG C sinter 1～
100h, more excellent is to sinter 2～50h at 1000～1100 DEG C；Thirdly, at a temperature of 450～650 DEG C
Ageing Treatment (Ageing Treatment refer to alloy workpiece after solution treatment, cold plastic deformation or casting, forging,
The heat treatment work of its performance, shape, size time to time change is kept in higher temperature placement or room temperature
Skill) 2～50h, more excellent is timeliness 4～20h at 450～500 DEG C, obtains sintering blank；Thirdly,
Sintering blank is processed into along maximal side a size of 100mm, is to the maximum along anisotropic orientation size
The sintered magnet of 10mm.
Afterwards, sintered magnet carrying out ultrasonic oil removing 30s successively, in dust technology, twice pickling 15s, dilute
Activation processing 15s in sulphuric acid, and deionized water cleaning can be standby, as being subject to processing sintered magnet.
In magazine, distributing mode is as shown in Figure 2.First, bottom magazine 2, one layer of heavy metal first it is paved with former
Material metal Dy bed material 5, shape can be tabular, graininess or powder；Secondly, at magazine 2
The high-melting-point powder particle 4 of interior addition zirconium oxide, silicon dioxide or alumina powder granule, interpolation
The particle diameter of high-melting-point powder particle 4 between 50～5000 μm, the height of high-melting-point powder particle after interpolation
Spend the height adjustable according to sintered magnet Yu magnetizing direction vertical direction, it is ensured that magnet can be completely buried in powder
In end；Thirdly, sintered magnet 3 is inserted into high-melting-point along the direction vertical with magnetizing direction
In powder particle 4, the upper end-face edge of magnet 3 is covered by powder completely, and ensures to be inserted into high-melting-point powder
Sintered magnet in the granule 4 of end does not contacts with the metal Dy bed material 5 bottom magazine, sintered magnet 3 simultaneously
Between do not contact each other；Thirdly, covering magazine lid 1, wherein magazine lid 1 is tight with the upper end of magazine 2
Contact, does not has clear gap.
In magazine, distributing mode can also be as shown in Figure 3.First, bottom magazine 7, metal Dy is first placed
Plate 10, the thickness of metal Dy plate is 1～5mm；Secondly, tile one layer on metal Dy plate 10
Particle diameter is 50～5000 μm zirconium oxides, silicon dioxide or alumina powder granule 9；Thirdly, exist
Sintered magnet 8, wherein sintered magnet 8 are placed on zirconium oxide, silicon dioxide or alumina powder granule
Magnetizing direction parallel with the short transverse of magazine, and do not contact each other between sintered magnet 8；Thirdly,
The one layer of particle diameter that tile on sintered magnet 8 is 50～5000 μm high-melting-point powder particles 9；Thirdly,
Repeat aforesaid operations, occupy magazine 7, enclosing cover feeding lid 6.
The magazine that will arrange metal Dy, powder and magnet puts into vacuum sintering furnace, at 750～1000 DEG C
Heat treatment 2～72h, more excellent is 800～950 DEG C for heat treatment temperature, and heat treatment time is 5～72h；
In vacuum sintering furnace, vacuum degree control is 10-2～10-55～20kPa are used in Pa or vacuum sintering furnace
Ar protective atmosphere, more excellent is 10 for vacuum-3～10-45～10kPa are used in Pa, or vacuum sintering furnace
Ar protective atmosphere, make metal Dy steam through zirconium oxide, silicon dioxide or alumina powder granule
Arrive sintered magnet surface, entered inside sintered magnet by grain boundary decision.
In this preparation method, if vacuum-sintering in-furnace temperature is less than 750 DEG C, due to the steam of metal Dy
Pressing through low, the Dy steam of generation can not effectively arrive sintered magnet surface and react with Grain-Boundary Phase,
Causing Dy to deposit in magnet surface, make top layer Dy concentration of element too high, center content is low even without Dy
The entrance of element；If temperature is higher than 1000 DEG C, Dy element can be diffused in crystal grain, makes sintering simultaneously
Magnet surface degradation, causes being greatly reduced of remanent magnetism and maximum magnetic energy product；And in cooling procedure Dy
Steam condenses in zirconium oxide, silicon dioxide or alumina powder in a large number, causes waste of raw materials.
In heat treatment diffusion process, if heat treatment time is less than 2h, sintered magnet surface distributed
Dy steam does not has the sufficient time to react with sintered magnet Grain-Boundary Phase, does not has grace time along Grain-Boundary Phase yet
Entering into sintered magnet center, thus cause sintered magnet top layer magnetic property apparently higher than center, magnet is equal
One property is deteriorated, and makes sintered magnet entirety magnetic property promote the highest simultaneously；If the process time is more than 72h,
Sintered magnet Dy steam distributed about can enter further in the principal phase of sintered magnet top layer, destroys main
Phase structure, thus cause sintered magnet magnetic property to be deteriorated.
Finally, after the time that above-mentioned process is implemented regulation, stop heating, make vacuum sintering furnace
Interior temperature is reduced under 200 DEG C；Restart heating afterwards, make vacuum-sintering in-furnace temperature be raised to
450～600 DEG C, more excellent is 470～550 DEG C；The process time is 1～10h, and more excellent is 2～5h.Treat
State after heat treatment implements the stipulated time, be passed through Ar air cooling in vacuum sintering furnace to room temperature.Afterwards will
Magazine takes out from sintering furnace, is taken out by sintered magnet, obtain R-Fe-B from high-melting-point powder particle
Based sintered magnet.
Embodiment 1
By neodymium, praseodymium, dysprosium, terbium, electrolytic iron, cobalt, copper, gallium, aluminum, zirconium, boron by weight: Nd-23.8%,
Pr-5%, Dy-0.6%, Tb-0.4%, Fe-68.29%, Co-0.5%, Cu-0.13%, Ga-0.1%, Al-0.1%,
The ratio of Zr-0.12%, B-1%, vacuum melting furnace in an inert atmosphere completes cast, cast temperature
Spending 1450 DEG C, chilling roller rotating speed is 60r/min, the flake thickness obtained about 0.3mm；Scale is through HD
Powder process, airflow milling, make the powder that particle mean size is 3.5 μm；Orientation pressure in the magnetic field of 15KOe
Make type, make pressed compact；Being put into by pressed compact in the sintering furnace under Ar atmosphere, 1100 DEG C of sintering 5h obtain
To green compact, green compact are timeliness 5h at a temperature of 500 DEG C, obtains sintering blank.Hair will be sintered by line cutting
Base is processed into the 50M magnet of a size of 40mm*20mm*4mm, is designated as M0。
Take the magazine A of three a size of 300mm*200mm*60mm, magazine B and magazine C, at the bottom of magazine A
Portion is paved with the Dy plate of a size of 50mm*50mm*2mm thickness, is paved with one layer of Dy granule (shape bottom magazine B
Shape is irregular, and granule maximum weight is less than 2g), it is paved with one layer of Dy powder (powder bottom magazine C
Particle diameter about 200 μm)；Zirconium oxide powder (powder diameter about 100 μm) is added afterwards in three magazines,
Zirconium oxide powder adds to distance magazine upper end-face edge 1cm.Then by 50M magnet through oil removing, acid
Washing, activate and after deionized water wash after dried, the direction along length 40mm is inserted vertically into
In Zirconium oxide powder, between magnet, be spaced 5mm, it is ensured that the lower end of magnet not with Dy metal evaporation sources
Contact, and the oxidized zirconium powder in upper end of magnet is completely covered.
Magazine A, B, C are placed in vacuum sintering furnace, at a temperature of 900 DEG C, (pressure under vacuum condition
10-3～10-4In the range of Pa) process 24h, afterwards Ageing Treatment 4h at 500 DEG C, logical Ar is cooled to
Room temperature.Magnet in magazine A, B and C is taken out, by the zirconium oxide on surface, silicon dioxide and oxidation
Aluminium powder processes clean, respectively obtains sintered magnet M1、M2And M3.Measured analysis, its performance is such as
Shown in table 1.
Table 1 M1、M2、M3And M0Comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | (g/cm3) | kGs | kOe | MGOe | - |
| M0 | 7.56 | 14.31 | 15.57 | 49.66 | 0.97 |
| M1 | 7.57 | 14.15 | 22.66 | 48.68 | 0.95 |
| M2 | 7.57 | 14.16 | 22.89 | 48.72 | 0.95 |
| M3 | 7.57 | 14.15 | 22.58 | 48.55 | 0.95 |
Pass through M0And M1、M2、M3Comparison of magnetic property, it can be seen that no matter use Dy plate, Dy
Grain or Dy powder, the magnetic property of the sintered magnet of heat treatment is significantly increased, and difference each other
Not quite.After process, the coercivity of 50M sintered magnet adds about 7kOe, and coercivity is increased dramatically,
Remanent magnetism, squareness and magnetic energy product slightly reduce；Owing to having processed 24h under 900 DEG C of high temperature, magnet
Density is slightly elevated.Take magnet surface and core sample spot after treatment and do energy spectrum analysis
(ICP-MS), result shows, in magazine A, B and C, sintered magnet composition is close, top layer Dy content
Increasing by 0.70%, center Dy content increases by 0.4%, shows that Dy permeates magnet the most completely.
Embodiment 2
Use and prepare with melting identical in embodiment 1, powder process, die mould, heat treatment and wire cutting method
50M magnetic sheet.
Take magazine D and E of two a size of 300mm*200mm*60mm, all spread bottom magazine D and E
The Dy plate of full a size of 50mm*50mm*2mm thickness, adds SiO 2 powder afterwards in magazine D
(powder diameter about 500 μm), addition silicon oxide pellets (a diameter of 3) in magazine E, two
In magazine, silicon dioxide all adds to distance magazine upper end-face edge 1cm.Then by 50M magnet through removing
After oil, pickling, activation and deionized water wash after dried, along the direction difference of length 40mm
It is inserted vertically in SiO 2 powder and bead, is spaced 5mm between magnet, it is ensured that under magnet
End does not contacts with Dy metal evaporation sources, and the oxidized zirconium powder in upper end of magnet is completely covered.
Magazine D and E is placed in vacuum sintering furnace, at a temperature of 850 DEG C, (pressure under vacuum condition
10-3～10-4In the range of Pa) process 48h, afterwards Ageing Treatment 5h at 550 DEG C, logical Ar is cooled to
Room temperature.Magnet in magazine D and E is taken out, magnet is processed clean, respectively obtain sintered magnet M4
And M5.Measured analysis, its performance is as shown in table 2.
Table 2 M4And M5With M0Comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | (g/cm3) | kGs | kOe | MGOe | - |
| M4 | 7.57 | 14.16 | 22.76 | 48.75 | 0.95 |
| M5 | 7.58 | 14.10 | 23.31 | 48.25 | 0.94 |
Pass through comparison of magnetic property, it can be seen that use the SiO 2 powder of powder and use zirconium oxide
Effect after powder heat treatment is essentially identical.After process, the coercivity of 50M sintered magnet adds about 7kOe,
Coercivity is increased dramatically, and remanent magnetism, squareness and magnetic energy product slightly reduce；Due at 850 DEG C of high temperature
Under processed 48h, the density of magnet is slightly elevated.After using globular silica-treated, Br relatively makes
Slightly reducing with powdered silica, it is big that Hcj increases quantitative change, and magnet density raises.This explanation is big
Particulate interspaces make more steam arrive sintered magnet surface, replace on sintered magnet surface.Take
Magnet surface and core sample spot do energy spectrum analysis (ICP-MS) after treatment, and result shows,
Sintered magnet M4Top layer Dy content increases by 0.70%, and center Dy content increases by 0.4%；Sintered magnet M5
Top layer Dy content increases by 0.90%, and center Dy content increases by 0.4%, shows that Dy permeates magnetic the most completely
Body.
Embodiment 3
Use and prepare with melting identical in embodiment 1, powder process, die mould, heat treatment and wire cutting method
50M magnetic sheet.
Take the magazine F of an a size of 300mm*200mm*60mm, be paved with a size of bottom magazine F
The Dy plate of 50mm*50mm*2mm thickness, (powder diameter is about to add alumina powder afterwards in magazine F
100 μm), alumina powder adds to distance magazine upper end-face edge 1cm.Then by 50M magnet warp
Cross after oil removing, pickling, activation and deionized water wash after dried, along the direction of length 40mm
It is inserted vertically into respectively in alumina powder and bead, is spaced 5mm between magnet, it is ensured that magnet
Lower end does not contacts with Dy metal evaporation sources, and the oxidized aluminium powder in upper end of magnet is completely covered.
Magazine F is placed in vacuum sintering furnace, at a temperature of 950 DEG C, (pressure 10 under vacuum condition-3~
10-4In the range of Pa) process 16h, afterwards Ageing Treatment 3h at 470 DEG C, logical Ar is cooled to room temperature.
Magnet in magazine F is taken out, obtains sintered magnet M6.Measured analysis, its performance such as table 3 institute
Show.
Table 3 M6With M0Comparison of magnetic property
Pass through comparison of magnetic property, it can be seen that use powder alumina powder and use zirconium oxide,
Effect after SiO 2 powder heat treatment is essentially identical.After process, the coercivity of 50M sintered magnet increases
About 7kOe, coercivity is increased dramatically, remanent magnetism, squareness and magnetic energy product slightly reduce；Due to
Having processed 16h under 950 DEG C of high temperature, the density of magnet is slightly elevated.Take after treatment magnet surface and in
Heart sample segment point does energy spectrum analysis (ICP-MS), and result shows, sintered magnet M6Top layer Dy content
Increasing by 0.70%, center Dy content increases by 0.3%, shows that Dy permeates magnet the most completely.
Embodiment 4
Use and prepare with melting identical in embodiment 1, powder process, die mould, heat treatment and wire cutting method
50M magnetic sheet.
Take the magazine G of an a size of 300mm*200mm*60mm, be paved with a size of bottom magazine G
The Dy plate of 50mm*50mm*2mm, is paved with alumina powder (powder size about 100 afterwards on Dy plate
μm), alumina powder thickness is 5mm, then by 50M magnetic sheet along thickness direction (magnetizing direction)
It is laid on alumina powder, on magnetic sheet, is again paved with the alumina powder of 5mm afterwards.Repeat above-mentioned
Operation is to filling magazine.
Magazine G is placed in vacuum sintering furnace, at a temperature of 950 DEG C, (pressure 10 under vacuum condition-3~
10-4In the range of Pa) process 16h, afterwards Ageing Treatment 3h at 470 DEG C, logical Ar is cooled to room temperature.
Magnet in magazine G is taken out, obtains sintered magnet M7.Measured analysis, its performance such as table 4 institute
Show.
Table 4 M7With M0Comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | (g/cm3) | kGs | kOe | MGOe | - |
| M7 | 7.57 | 14.21 | 23.80 | 48.95 | 0.96 |
Pass through comparison of magnetic property, it can be seen that use Dy plate, alumina powder and magnet alternately to place
The sintered magnet M that after heat treatment obtains of method7Magnetic property, whether remanent magnetism, coercivity or magnetic
Energy product, with M6Essentially identical.After process, 50M sintered magnet is compared with before process, and coercivity adds about
7kOe, remanent magnetism, squareness and magnetic energy product slightly reduce；Owing to having processed 16h under 950 DEG C of high temperature,
The density of magnet is slightly elevated.Take magnet surface after treatment and core sample spot is done power spectrum and divided
Analysis (ICP-MS), result shows, sintered magnet M7Top layer Dy content increases by 0.80%, and center Dy contains
Amount increase by 0.3%, shows that Dy permeates magnet the most completely.
Embodiment 5
By neodymium, praseodymium, dysprosium, terbium, electrolytic iron, cobalt, copper, gallium, aluminum, zirconium, boron by weight: Nd-24.3%,
Dy-5.7%, Fe-66.52%, Co-2%, Cu-0.18%, Ga-0.08%, Al-0.15%, B-0.97%'s
Ratio, vacuum melting furnace in an inert atmosphere completes cast, pouring temperature 1470 DEG C, chilling roller
Rotating speed is 50r/min, the flake thickness obtained about 0.25mm；Scale through HD powder process, airflow milling,
Make the powder that particle mean size is 3.3 μm；The magnetic field of 15KOe is orientated compressing, makes pressure
Base；Being put into by pressed compact in the sintering furnace under Ar atmosphere, 1080 DEG C of sintering 6h obtain green compact, and green compact exist
Timeliness 4h at a temperature of 490 DEG C, obtains sintering blank.By line cutting, sintering blank is processed into a size of
The 42S magnet of 40mm*20mm*4mm, is designated as S0。
Take the magazine H of three a size of 300mm*200mm*60mm, magazine I and magazine J, at the bottom of magazine H
Portion is paved with the Dy plate of a size of 50mm*50mm*2mm thickness, is paved with one layer of Dy granule (shape bottom magazine I
Shape is irregular, and granule maximum weight is less than 2g), it is paved with one layer of Dy powder (powder bottom magazine J
Particle diameter about 2000 μm)；Zirconium oxide powder (powder diameter about 1000 μ is added afterwards in three magazines
M), Zirconium oxide powder adds to distance magazine upper end-face edge 1cm.Then by 42S magnet through removing
After oil, pickling, activation and deionized water wash after dried, vertical along the direction of length 40mm
Be inserted in Zirconium oxide powder, between magnet, be spaced 5mm, it is ensured that the lower end of magnet not with Dy metal
Evaporation source contacts, and the oxidized zirconium powder in upper end of magnet is completely covered.
Magazine H, I, J are placed in vacuum sintering furnace, at a temperature of 950 DEG C, (pressure under vacuum condition
10-3～10-4In the range of Pa) process 16h, afterwards Ageing Treatment 4h at 500 DEG C, logical Ar is cooled to
Room temperature.Magnet in magazine H, I and J is taken out, by the zirconium oxide on surface, silicon dioxide and oxidation
Aluminium powder processes clean, respectively obtains sintered magnet S1、S2And S3.Measured analysis, its performance is such as
Shown in table 5.
Table 5 S1、S2、S3And S0Comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | (g/cm3) | kGs | kOe | MGOe | - |
| S0 | 7.55 | 12.85 | 23.15 | 41.50 | 0.95 |
| S1 | 7.57 | 12.80 | 29.62 | 41.38 | 0.93 |
| S2 | 7.57 | 12.82 | 30.01 | 41.26 | 0.93 |
| S3 | 7.57 | 12.80 | 29.47 | 41.22 | 0.93 |
Pass through S0And S1、S2、S3Comparison of magnetic property, it can be seen that no matter use Dy plate, Dy
Grain or Dy powder, the magnetic property of the sintered magnet of heat treatment is significantly increased, and difference each other
Not quite.After process, the coercivity of 42S sintered magnet adds 6～7kOe, and coercivity is increased dramatically,
Remanent magnetism is basically unchanged, and squareness slightly reduces；Owing to having processed 16h under 950 DEG C of high temperature, magnet
Density is slightly elevated.Take magnet surface and core sample spot after treatment and do energy spectrum analysis
(ICP-MS), result shows, in magazine H, I and J, sintered magnet composition is close, top layer Dy content
Increasing by 0.70%, center Dy content increases by 0.4%, shows that Dy permeates magnet the most completely.
The foregoing is only the better embodiment of the present invention, not in order to limit the present invention, all at this
Within bright spirit and principle, any modification, equivalent substitution and improvement etc. made, should be included in this
Within the protection domain of invention.
Claims (8)
1. a preparation method for R-Fe-B based sintered magnet, including:
1) R is prepared1-Fe-B-M sintered magnet, wherein, R1Selected from Nd, Pr, Dy, Tb, Ho, Gd
In one or several, its total amount is 26wt%～33wt%；M selected from Ti, V, Cr, Mn, Co,
One or several in Ni, Ga, Ca, Cu, Zn, Si, Al, Mg, Zr, Nb, Hf, Ta, W, Mo
Kind, its total amount is 0～5wt%；B total amount is 0.5wt%～2wt%；Remaining is Fe；
2) by step 1) sintered magnet that obtains carries out at oil removing, pickling, activation and deionized water cleaning
Reason；
3) by step 2) in clean after sintered magnet be inserted into along the direction vertical with magnetizing direction and fill out
Have in the magazine of high-melting-point powder particle, wherein first at magazine before filling described high-melting-point powder particle
Bottom is paved with metal Dy bed material；Or, according to metal Dy plate, high-melting-point powder particle, sintered magnet,
The order of high-melting-point powder particle is during stratiform is placed in magazine successively, wherein sintered magnet magnetizing direction and material
Box short transverse is parallel；
4) by step 3) in hold the magazine of sintered magnet, high-melting-point powder particle and metal Dy and put into
In vacuum sintering furnace, heat treatment 2～72h in 750～1000 DEG C, vacuum degree control in vacuum sintering furnace
10-2～10-5Use the Ar protective atmosphere of 5～20kPa in Pa or vacuum sintering furnace, make metal Dy
Steam is entered inside sintered magnet by grain boundary decision；
5) by step 4) process after sintered magnet in 450～600 DEG C of Ageing Treatment 1～10h, obtain
R-Fe-B based sintered magnet；
Wherein, step 3) in the described metal Dy bed material that is paved with bottom magazine be tabular, graininess or
Powder.
Preparation method the most according to claim 1, it is characterised in that: in step 3) in, work as burning
Knot magnet is inserted into along the direction vertical with magnetizing direction when being filled with in the magazine of high-melting-point powder particle,
The height of the described high-melting-point powder particle added is on the sintered magnet direction vertical with magnetizing direction
Highly it is set to ensure that magnet can be completely buried in described high-melting-point powder particle.
Preparation method the most according to claim 1, it is characterised in that: in step 3) in, work as burning
Knot magnet is inserted into along the direction vertical with magnetizing direction when being filled with in the magazine of high-melting-point powder particle,
Sintered magnet does not contacts with the metal bed material bottom magazine, does not contacts each other between sintered magnet simultaneously.
Preparation method the most according to claim 1, it is characterised in that: in step 3) in, when pressing
According to metal Dy plate, high-melting-point powder particle, sintered magnet, the order layer successively of high-melting-point powder particle
When shape is placed in magazine, the thickness of the described high-melting-point powder particle of interpolation is 1～50mm.
Preparation method the most according to claim 4, it is characterised in that: the described high-melting-point of interpolation
The thickness of powder particle is 1～20mm.
6. according to the arbitrary described preparation method of claim 1 to 5, it is characterised in that: described Gao Rong
Point powder particle is any one in zirconium oxide, silicon dioxide or alumina powder granule, and particle diameter exists
Between 50～5000 μm.
7. according to the arbitrary described preparation method of claim 1 to 5, it is characterised in that: in step 4)
In, vacuum-sintering in-furnace temperature is 800～950 DEG C, and heat treatment time is 5～72h, vacuum sintering furnace
Interior vacuum is 10-3～10-4Pa；Or use the Ar protective atmosphere of 5～10kPa in vacuum sintering furnace.
8. according to the arbitrary described preparation method of claim 1 to 5, it is characterised in that: in step 5)
In, described aging temperature is 470～550 DEG C, and the process time is 2～5h.
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| JP5880448B2 (en) * | 2011-01-19 | 2016-03-09 | 日立金属株式会社 | Method for producing RTB-based sintered magnet |
| CN103985535A (en) * | 2014-05-31 | 2014-08-13 | 厦门钨业股份有限公司 | Method for conducting Dy diffusion on RTB-system magnet, magnet and diffusion source |
| CN104240883B (en) * | 2014-09-12 | 2016-10-05 | 沈阳中北通磁科技股份有限公司 | RE permanent magnetic alloy sheet and dual alloy Nd-Fe-B permanent magnet and manufacture method thereof |
| CN105469973B (en) * | 2014-12-19 | 2017-07-18 | 北京中科三环高技术股份有限公司 | A kind of preparation method of R T B permanent magnets |
| CN105321701B (en) * | 2015-07-01 | 2018-08-24 | 浙江东阳东磁稀土有限公司 | A kind of the dress firing method and device of rare-earth Nd-Fe-B magnet |
| CN105185498B (en) * | 2015-08-28 | 2017-09-01 | 包头天和磁材技术有限责任公司 | Rare earth permanent-magnet material and its preparation method |
| CN106128678B (en) * | 2016-08-17 | 2018-02-16 | 宁波永久磁业有限公司 | A kind of method for preparing R T B rare-earth permanent magnets |
| CN106298135B (en) * | 2016-08-31 | 2018-05-18 | 烟台正海磁性材料股份有限公司 | A kind of manufacturing method of R-Fe-B sintered magnet |
| CN107147228A (en) * | 2017-03-23 | 2017-09-08 | 烟台正海磁性材料股份有限公司 | The preparation method and rotor for electromotor of a kind of Sintered NdFeB magnet |
| CN107578912A (en) * | 2017-09-25 | 2018-01-12 | 烟台正海磁性材料股份有限公司 | A kind of preparation method of the neodymium iron boron magnetic body with high-coercive force |
| CN110090952A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of the dress firing method and device of rare-earth Nd-Fe-B magnet |
| CN111489888B (en) * | 2019-01-28 | 2024-01-02 | 株式会社博迈立铖 | Method for producing R-T-B sintered magnet |
| TWI693206B (en) * | 2019-03-08 | 2020-05-11 | 中國鋼鐵股份有限公司 | Method of fabricating modified ferrite magnetic powder and method of fabricating ferrite magnet |
| CN112750613B (en) * | 2020-03-31 | 2023-02-07 | 河北泛磁聚智电子元件制造有限公司 | Preparation method of ultrahigh maximum magnetic energy product sintered samarium-cobalt magnet |
| CN111430090B (en) * | 2020-04-21 | 2023-04-07 | 福建省长汀金龙稀土有限公司 | Neodymium-iron-boron magnet material and preparation method and application thereof |
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| CN114042921B (en) * | 2021-11-16 | 2024-03-22 | 宁波江丰电子材料股份有限公司 | Chromium-silicon alloy powder and preparation method and application thereof |
| CN115036089B (en) * | 2022-07-07 | 2023-04-07 | 宁波迈泰克磁材科技有限公司 | High-temperature-resistant neodymium-iron-boron magnetic steel for vehicle-mounted main motor and preparation method thereof |
| CN116479487B (en) * | 2023-06-07 | 2024-06-14 | 宁波科宁达工业有限公司 | Electroplated magnet and method for preparing same |
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